• Title, Summary, Keyword: 유도체화

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Comparison of isoButoxycarbonyl derivatives, tert.-butyldimethylsilyl derivatives, with US EPA Method in the sensitivity of Alkylphenols, Chlorophenols, and Bisphenol A Potential field-screening applications of GC/MS-SIM (기체 크로마토그래피/질량분석기를 이용한 field-screening 적용을 위한 알킬페놀류, 클로로페놀류 및 비스페놀 A의 isoBOC 유도체, TBDMS 유도체와 US EPA 방법의 비교)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.196-213
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    • 2002
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison; EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1~109.9% (EPA method) and 90.3~126.6% (isoBOC derivatization and TBDMS derivatization), respectively. The method detection limit of bisphenol A for SIM were 0.732 ${\mu}g/{\ell}$ (EPA method), 0.002 ${\mu}g/{\ell}$ (isoBOC derivatization) and 0.021 ${\mu}g/{\ell}$ (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755~0.9981 (isoBOC derivatization), and 0.9908~0.9996 (TBDMS derivatization). When these methods were applied to treated wastewater sample from a polyethylene plant, the concentrations of 11 phenols were below the method detection limit.

Effects of Conjugated Double Bond Derivatives of Polyunsaturated Fatty Acid on Serum Lipids in Rats (다가불포화지방산의 공역이중결합 유도체가 흰쥐의 혈청 지질 성분에 미치는 영향)

  • Kim, So-Young;Kim, Sung-Hee;Kim, Gyeong-Eup
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.9
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    • pp.1120-1127
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    • 2007
  • This study was designed to examine the effects of n-6 PUFA rich corn oil, n-3 PUFA rich perilla oil and their conjugated double bond derivatives on serum lipids status in rats. Experimental diets containing lard (control), corn oil (CO), perilla oil (PO), conjugated double bond derivatives of n-6 PUFA rich corn oil (TCO) and n-3 PUFA rich perilla oil (TPO) at the level of 10% (w/w) were fed to male Sprague Dawley rats for 4 weeks. TCO was found to have three derivatives of linoleic acid and TPO had five derivatives of linolenic acid by GC. Serum total cholesterol levels were significantly lower in the all experimental groups than in the control group, and particularly, the lowest in TCO and TPO groups. HDL-cholesterol concentrations were a little higher in the all experimental groups than in the control group, and TCO and TPO groups were not significantly different from CO and PO groups. Serum LDL, LDL-cholesterol, chylomicron and triglyceride concentrations were significantly lower in the all experimental groups than in the control group, remarkably lower in TCO group and particularly, the lowest in the TPO group. Serum free cholesterol and cholesteryl ester concentrations were lower in TCO and TPO groups than in CO and PO groups. From the above research, TCO and TPO groups were effective on the improvement of the lipid compositions in serum and particularly, TPO group was the most effective on the improvement of serum lipids.

Analysis of gibberellic acid from fruits using HPLC/UV-vis (HPLC/UV-vis을 이용한 과일류 중의 지베렐린 산 분석)

  • Ma, Kyung Na;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.19-26
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    • 2013
  • Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.

Determination of Trace Amounts of Formaldehyde in Water Using High Performance Liquid Chromatography and Acetylacetone as a Derivative Reagent (아세틸아세톤 유도체화 시약과 HPLC를 이용한 미량 포름알데하이드 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.2
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    • pp.81-86
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    • 2015
  • A simple analytical method to quantify formaldehyde in water at lower levels (${\mu}g/L$) was developed using a high performance liquid chromatography (HPLC) and acetylacetone as a derivative reagent. Unlike conventional methods, no extraction and/or concentration were required. The derivative reagent was added into samples and reacted for 30 minutes at $80^{\circ}C$ prior to the analysis of formaldehyde using HPLC. The method detection limit and the limit of quantification for this method were 1.6 and $5.0{\mu}g/L$, respectively. This method also achieved high precision (0.6-3.0%) and accuracy (91.6-106.3%). The recovery rates for various environmental samples ranged from 92.0 to 115.2%.

Determination of the Concentration of Panaxynol, Panaxydol and Panaxytrio1 by Capillary-GC(FID) (Capillary-GC(FID)에 의한 panaxynol, panaxydol 및 panaxytriol의 정량)

  • 노길봉;손현주
    • Journal of Ginseng Research
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    • v.13 no.2
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    • pp.183-188
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    • 1989
  • A gas chromatographic method was developed for determination of the concentration of three major polyacetylene compounds in ginseng roots---panaxynol, panaxydol and panaxytriol. The column and the detector used were an SPB-1 fused silica capillary (0.2mm i.d.$\times$30m, Supelco) and a flame ionization detector (FID). The column oven temperature was kept at $250^{\circ}C$ isothermally The retention times of panaxynol, panaxydol and panaxytriol peaks were 4.2,5.1 and 6.9 min before TMS-derivatitration and 4.5,5.4 and 7.4 min after TMS-derivatization, respectively. The minimum determinable concentrations of panaxynol, panaxydol and panaxytriol before TMS-derivatiEation were at the 20, 50 and 100 ppm levels, while the concentrations of panaxydol and panaxytriol as well as panaxynol after TMS- derivatisation could be towered to the 5 ppm level. The panaxynol, panaxydol and panaxytriol contents in red ginseng were determined by use of this method after TMS-derivatization : the amounts obtained were 724, 721 and 71$\mu\textrm{g}$/g, respectively.

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Analysis of derivatized MX by Gas Chromatography/Mass Spectrometry (GC/MS를 이용한 MX 유도체화 분석법 연구)

  • Yoo, Eun-Ah;Park, Do-Yeon;Lee, Hyang-Ki;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.221-228
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    • 2002
  • AMX is one of extremely high mutagenic compound produced from the reaction of the chlorine and the organic compound during the disinfection of tap water. In this paper, the chemical derivatization of MX with 2% sulfuric acid-methanol, iso-propanol, sec-butanol and n-butanol derivatives for the GC/MS analysis were tested or compared. Limit of detection for the EI and NCI mode were 25 pg and 1.25 pg, respectively. The good linear calibration curve was obtained the range of 25~2500 pg by EI and NCI

DEVELOPMENT AND COMPARISION OF RESIDUE ANALYSIS FOR BENOMYL IN BEAN AND BEAN SPROUTS (두류와 콩나물에서의 BENOMYL의 검색과 그 분리에 관한 연구)

  • Han, Ilkeun;Chai, Jeungyoung;Lee, Jayoung;Yeo, Ikhyun
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.395-402
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    • 1994
  • Benomyl(Methyl-1-(Butyl Carbamoyl)-Benzimidazole-2-yl-Carbamate) is widely used as pre- and post-harvest pesticide. It converts into MBC(Carbendarzime:Benzimidazole-2-yl-carbamate) and butyl-isocyanate in mild condition. In this study, three analytical methods for MBC were compared in view of detectability, correctness, and sensitivity. The first and second are HPLC analytical method employing the UV detection of MBC. Our new third method was modification of PFBB(pentafluoro-benzylbromide) derivatization method with GC-ECD & MSD. The average recoveries and detection limit of MBC in the newly modified method are 95% and $0.001{\mu}g/g$ in whole bean and bean sprouts respectively. This new method prevent pesticide analysis from misdetecting in bean and bean sprouts.

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Applied Analysis for Metabolic Profiling of Trace-level Amino Acid in Biological Fluid (생체시료 중 미량 아미노산 대사 프로필을 위한 분석법 응용)

  • Nam, Hyung Wook;Park, Song-Ja;Pyo, Hee Soo;Paeng, Ki Jung
    • Analytical Science and Technology
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    • v.16 no.5
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    • pp.349-357
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    • 2003
  • The universality of low molecular weight metabolites (i.e. amino acids, steroid hormones) allows rapid and straightforward investigation of biochemistry of genetically un-characterized species. Thus in vivo metabolic profiling of amino acid in combination with multivariate data analysis (metabolomics) offers great potential in comparative biology. In this paper, amino acid profiles in biological fluid (media) were studied by using HPLC/FLD. HPLC procedure for amino acids require the formation of derivatives due to the low absorption of the free compounds. o-Phthalaldehyde (OPA) used in association with a thiol, such as 3-mercaptopropionic acid (3-MPA), is one of the most popular and sensitive reagents, which yield quickly fluorescent iso-indoles at room temperature. To improve unstability of OPA/3-MPA derivatization, we optimized injector programs for fixed injection times. Linear regressions for the standard curves were linear in the range 0.5 - 100.0 ppb, giving correlation coefficents above 0.99. The detection limit were 1.70 pmol(GLU) - 23.81 pmol(SER). It is practically useful when the amount of sample is very low on single cells.

Derivatization and Residual Determination of MCPP in Soil Leachate (토양 침투수중 MCPP의 유도체화 및 잔류분석)

  • Hong, Moo-Ki;Smith, Albert E.
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.199-208
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    • 1994
  • Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

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